• Proceedings of the Korean Institute of Surface Engineering Conference
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• 2014.11a
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• pp.304-304
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• 2014

Quaternary Ti-Al-Si-N films were deposited on WC-Co substrates by a hybrid deposition system of arc ion plating (AIP) method for Ti-Al source and DC magnetron sputtering technique for Si incorporation. The synthesized Ti-Al-Si-N films were revealed to be composites of solid-solution (Ti,Al)N crystallites and amorphous $Si_3N_4$ by instrumental analyses. The Si addition in Ti-Al-N films affected the refinement and uniform distribution of crystallites by percolation phenomenon of amorphous silicon nitride, similarly to Si effect in TiN film. As the Si content increased up to about 9 at.%, the hardness of Ti-Al-N film steeply increased from 30 GPa to about 50 GPa. The highest microhardness value (~50 GPa) was obtained from the Ti-Al-Si-N film having the Si content of 9 at.%, the microstructure of which was characterized by a nanocomposite of $nc-(Ti,Al)N/a-Si_3N_4$.

• Proceedings of the Korean Vacuum Society Conference
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• 1999.07a
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• pp.211-211
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• 1999

Titanium nitride (TiN) thin films have useful properties including high hardness, good electrical conductivity, high melting point, and chemical inertness. The applications have included wear-resistant hard coatings on machine tools and bearings, decorative coating making use of the golden color, thermal control coatings for widows, and erosion resistant coatings for spacecraft plasma probes. For all these applications as feature sizes shrink and aspect ratios grow, the issue of good step coverage becomes increasingly important. It is therefore essential to manufacture conformal coatings of TiN. The growth of TiN thin films by chemical vapor deposition (CVD) is of great interest for achieving conformal deposition. The most widely used precursor for TiN is TiCl4 and NH3. However, chlorine impurity in the as-grown films and relatively high deposition temperature (>$600^{\circ}C$) are considered major drawbacks from actual device fabrication. To overcome these problems, recently, MOCVD processes including plasma assisted have been suggested. In this study, therefore, we have doposited Ti(C, N) thin films on Si(100) and D2 steel substrates in the temperature range of 150-30$0^{\circ}C$ using tetrakis diethylamido titanium (TDEAT) and titanium isopropoxide (TIP) by pulsed DC plamsa enhanced metal-organic chemical vapor deposition (PEMOCVD) method. Polycrystalline Ti(C, N) thin films were successfully grown on either D2 steel or Si(100) surfaces at temperature as low as 15$0^{\circ}C$. Compositions of the as-grown films were determined with XPS and RBS. From XPS analysis, thin films of Ti(C, N) with low oxygen concentration were obtained. RBS data were also confirmed the changes of stoichiometry and microhardness of our films. Radical formation and ionization behaviors in plasma are analyzed by optical emission spectroscopy (OES) at various pulsed bias and gases conditions. H2 and He+H2 gases are used as carrier gases to compare plasma parameter and the effect of N2 and NH3 gases as reactive gas is also evaluated in reduction of C content of the films. In this study, we fond that He and H2 mixture gas is very effective in enhancing ionization of radicals, especially N resulting is high hardness. The higher hardness of film is obtained to be ca. 1700 HK 0.01 but it depends on gas species and bias voltage. The proper process is evident for H and N2 gas atmosphere and bias voltage of 600V. However, NH3 gas highly reduces formation of CN radical, thereby decreasing C content of Ti(C, N) thin films in a great deal. Compared to PVD TiN films, the Ti(C, N) film grown by PEMOCVD has very good conformability; the step coverage exceeds 85% with an aspect ratio of more than 3.

• Journal of the Korean Ceramic Society
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• v.35 no.11
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• pp.1130-1140
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• 1998

Thin films of $Bi_4Ti_3O_{12}\;nBaTiO_3(n=1&2)$ were prepared using sols erived Ba-Bi-Ti complex alkoxides. The sols were spin-cast onto $Pt/Ti/SiO_2/Si$ substrates and followed by pyrolysis for 1 hr at $620^{\circ}C,\;700^{\circ}C\;and\;750^{\circ}C$ In the thin films a pyrochlore phase seemed to be formed at a lower temperature and then tran-formed to the layered perovskite phase as the heating temperature increased. In the thin films pyrolyzed at formed to the layered perovskte phase as the heating temperature increased. In the films pyrolyzed at $750^{\circ}C$ the amount of $Bi_4Ti_3O_{12}{\cdot}BaTiO_3$ reached to 94% while $Bi_4Ti_3O_{12}{\cdot}BaTiO_3$ was 77% in composition. This result shows that the formation of the layered pervoskite phase becomes difficult as the amount of complexing $BaTiO_3$ increases. The microstructures and the electrical properties of the thin films were gen-erally improved with the incease of the heating temperature. However the presence of the pyrochlore phase could not be removed effectively. Our study showed that the electrical properties of $Bi_4Ti_3O_{12}{\cdot}BaTiO_3$ were pronouncedly improved with complexing with BaTiO3 when compared to those of $Bi_4Ti_3O_{12}$ while the presence of the pyrochlore phase was detrimental to the those of $Bi_4Ti_3O_{12}{\cdot}2BaTiO_3$.

• Journal of the Korean Society for Heat Treatment
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• v.17 no.4
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• pp.236-240
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• 2004

Effect of plasma power on PECVD process were investigated in this study. TiN and TiCN films were deposited on nitrided STD11 steel with 600W, 1,200W and 1,600W plasma power. As the plasma power was increased, the preferred orientation was reinforced from (200) to (111) and the hardness of films was improved. The low plasma power was, however, effective for improving of adhesion force of films. Regarding above properties, TiN and TiCN films were deposited by gradient plasma power. It was possible to get high hardness as well as adhesion force through gradient plasma power.

• Journal of Surface Science and Engineering
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• v.38 no.6
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• pp.207-211
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• 2005

In this work a multi-layered nanostructured TiAIN/CrN superlattice coatings was synthesized using closed-field unbalanced magnetron sputtering method and the relationships between their superlattice period (1), micro-structure, hardness and elastic modulus were investigated. In addition, wear test at $500^{\circ}C$ and oxidation resistance test at $900^{\circ}C$ were performed to investigate high temperature properties of these thin films. The coatings were characterized in terms of microstructure and mechanical properties by transmission electron microscopy (TEM) and nano-indentation test. Results from TEM analysis showed that superlattice periods was inversely proportional to the jig rotation speed. The maximum hardness and elastic modulus of 37 GPa and 375 GPa were observed at superalttice period of 6.1 nm and 4.4 nm, respectively. An higher value of microhardness from TiAIN/CrN thin films than either TiAIN (30 GPa) or CrN (26 GPa) was noted while the elastic modulus was approximately an average of TiAIN and CrN films. These enhancement effects in superlattice films could be attributed to the resistance to dislocation glide across interface between the CrN and TiAIN layers. Much improved plastic deformation resistance ($H^3/E^2$) of 0.36 from TiAIN/CrN coatings was observed, compared with 0.15 and 0.16 from TiAIN and CrN, respectively. Also the wear resistance at $500^{\circ}C$ was largely increased than those of single TiAIN and CrN coatings and TiAIN/CrN coatings showed much reduced weight gain after exposure at $900^{\circ}C$ for 20 hours.

• Journal of the Korean Vacuum Society
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• v.6 no.3
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• pp.255-262
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• 1997

Titanium nitride (TiN) films were prepared by reactive sputter deposition in mixed gas of Ar+$N_2$. The volume percentage of $N_2$ in the working gas was chosen so as to grow stoichiometric TiN films and the substrate temperature during film growth was set from room temperature to $700^{\circ}C$. Stoichiometric $Ti_{0.5}N){0.5}$ films with (111) texture were grown at temperatures over $600^{\circ}C$, while films prepared at temperatures below $600^{\circ}C$ showed N-rich TiN. The composition X and y in the $Ti_xN_y$ films determined by XPS and RBS varied within 5% with the substrate temperature. The sheet resistance of the TiN films decreases as the substrate temperature increased. TiN film prepared at $600^{\circ}C$ showed 14.5$\Omega\Box$, and it decreased to 8.9$\Omega\Box$ after the sample was annealed at $700^{\circ}C$, 30 sec in Ar-gas ambient by RTA. By far, high quality stoichiometric TiN films by reactive sputtering in the mixed gas ambient could be prepared at substrate temperature over $600^{\circ}C$.

• Journal of the Korean Ceramic Society
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• v.47 no.6
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• pp.479-484
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• 2010

Microstructural and mechanical properties of the TiN films deposited on Si substrates under various substrate bias voltages by a reactive magnetron sputtering have been studied. It was found that the crystallographic texture, microstructural morphology and mechanical property of the TiN films were strongly depended on the substrate bias voltage. TiN films deposited without bias exhibited a mixed (200)-(111) texture with a strong (200) texture, which subsequently changed to a strong (111) texture with increasing bias voltage. It is also observed that the crystallite size decreases with increasing bias voltage, which corresponds to the increasing diffraction peak width of XRD patterns. The average surface roughness was calculated from AFM images of the films; these results indicated that the average surface roughness was increased with an increase in the bias voltage of the coatings.

• Journal of Surface Science and Engineering
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• v.42 no.5
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• pp.203-207
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• 2009

Interaction between human osteoblast (hFOB 1.19) and CrN films was conducted in vitro. CrN films were produced by cathodic arc plasma deposition. The surface was characterized by atomic force microscopy (AFM). CrN films, glass substrates and TiN films were cultured with human osteoblasts for 48 and 72 hours. Actin stress fiber patterns and cell adhesion of osteoblasts were found less organized and weak on CrN films compared to those on the glass substrates and the TiN films. Human osteoblasts also showed less proliferation and less distributed microtubule on CrN films compared to those on glass substrates and TiN films. Focal contact adhesion was not observed in the cells cultured on CrN films, whereas focal contact adhesion was observed well in the cells cultured on glass substrates and TiN films. As a result, the CrN film is a potential candidate as a surface coating to be used for implantable devices which requires minimal cellular adhesion.

• Journal of Surface Science and Engineering
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• v.39 no.2
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• pp.70-75
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• 2006

As technology advances, there is a demand for development of hard, solid lubricant coating. (Ti,Cr)N-$MoS_2$, films were deposited on SKD 11 tool steel substrate by co-deposition of $MoS_2$, with (Ti,Cr)N using a D.C. magnetron sputtering process. The influence of the $N_2/Ar$ gas ratio, the deposition temperature, the amount of $MoS_2$ in the films, and the bias voltage on the mechanical and the structural properties of the films were investigated. Wear tests were performed on the films deposited in various conditions.

• Journal of the Korean Ceramic Society
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• v.31 no.7
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• pp.731-738
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• 1994

TiN films were deposited on high speed steels by plasma assisted chemical vapor deposition (PACVD), cathode arc ion plating (CAIP) and reactive magnetron sputtering (RMS). The properties of the films deposited by the three different methods were compared. The preferred oriented plane of PACVD-TiN is (200) and those of CAIP-TiN and RMS-TiN are (111). PACVD-TiN shows a dome surface and a microstructure having small grains. CAIP-TiN shows the highest microhardness and the best adhesion strength of the three because it has a dense microstructure and an ill-defined interface. But is shows the greatest surface roughness due to the Ti droplet created by the arc. RMS-TiN shows a microstructure having large voids so that its properties in microhardness and adhesion are the worst of the three.